Method for separating borneol by using separation kettle with stirrer of supercritical CO2 fluid extraction system

A separation kettle and supercritical technology, applied in the separation/purification of hydroxyl compounds, bulk chemical production, organic chemistry, etc., can solve the problems of large production field occupation, hidden danger of borneol safety, low efficiency, etc. The effect of short purification time and low loss

Inactive Publication Date: 2010-07-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Problems existing in the current process: first, gasoline is used as a solvent in the two crystallization and purification of crude borneol, and gasoline belongs to Class A flammable liquid, which brings great safety hazards to the generation of borneol, and because gasoline Volatile, causing great pollution to the air environment
Second, the crystallization process takes a long time, and it takes about 12 days to crystallize and purify a qualified borneol product. The product production cycle is long, and the crystallization yield is greatly affected by the temperature, and the efficiency is extremely low.
Third, since borneol is a medicinal raw material, solvent gasoline is difficult to remove in the final drying process, and the residue of gasoline will cause certain risks to the quality of the drug
Fourth, due to the long production cycle, the production site occupies a large area, and the loss of solvent is serious, resulting in extremely high production costs

Method used

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  • Method for separating borneol by using separation kettle with stirrer of supercritical CO2 fluid extraction system
  • Method for separating borneol by using separation kettle with stirrer of supercritical CO2 fluid extraction system
  • Method for separating borneol by using separation kettle with stirrer of supercritical CO2 fluid extraction system

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Weighing a certain batch of thick borneol 250g, its orthoborneol content is 44%, directly this borneol is put into extraction kettle 1, pressurizes CO by high-pressure pump 7 2 The fluid passes through the heat exchanger to make CO 2 The fluid becomes subcritical fluid and enters the extraction kettle 1 from the bottom of the extraction kettle for extraction, and the extraction condition is extraction pressure 16MP a , the extraction temperature is 25°C.

[0032] (2) The fluid containing orthoborneol and other components extracted by the extraction kettle enters the middle part of the separation column 2, and performs first-stage separation in the separation column. Separation column pressure 10MP a , temperature 5°C;

[0033] (3) the fluid that has concentrated orthoborneol through the first-stage separation column 1 enters the separation kettle 3 again, and carries out second-stage separation in the separation kettle, and the separation kettle pressure is 7MP ...

Embodiment 2

[0037](1) weighing a certain batch of thick borneol 250g, its orthoborneol weight content is 44%, directly this borneol enters in the extraction kettle 1, is pressurized by high-pressure pump 7 and CO 2 The fluid passes through the heat exchanger to make CO 2 The fluid becomes supercritical fluid and enters the extraction kettle 1 from the bottom of the extraction kettle for extraction, and the extraction condition is extraction pressure 30MP a , The extraction temperature is 45°C.

[0038] (2) The fluid containing orthoborneol and other components extracted by the extraction kettle enters the middle part of the separation column 2, and performs first-stage separation in the separation column. Separation column pressure 16MP a , temperature 35°C;

[0039] (3) The fluid that has concentrated orthoborneol through the first-stage separation column 1 enters the separation kettle 3 again, and carries out second-stage separation in the separation kettle, and the separation kettle...

Embodiment 3

[0043] (1) weighing a certain batch of thick borneol 250g, its orthoborneol content is 44%, directly enters in the extraction kettle 1, is pressurized by the high-pressure pump 7 and CO 2 The fluid passes through the heat exchanger to make CO 2 The fluid becomes supercritical fluid and enters the extraction kettle 1 from the bottom of the extraction kettle for extraction, and the extraction condition is extraction pressure 30MP a , The extraction temperature is 45°C.

[0044] (2) The fluid containing orthoborneol and other components extracted by the extraction kettle enters the middle part of the separation column 2, and performs first-stage separation in the separation column. Separation column pressure 16MP a , temperature 35°C;

[0045] (3) The fluid that has concentrated orthoborneol through the first-stage separation column 1 enters the separation kettle 3 again, and carries out second-stage separation in the separation kettle, and the separation kettle pressure is 9M...

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Abstract

The invention discloses a method for separating borneol by using a separation kettle with a stirrer of a supercritical CO2 fluid extraction system. In the method, CO2 is used as a solvent to dissolve crude borneol, the separation kettle with the stirrer is designed for separating and purifying the borneol, and a relatively pure borneol product can be obtained by separating with violent stirring. The method comprises the following steps: putting the crude borneol (solid) to an extraction kettle for extracting, wherein the extraction process is in a subcritical or supercritical environment under the extraction pressure of between 6 and 35MPa and at the extraction temperature of between 25 and 90 DEG C; performing primary separation in a separation column under the pressure of between 6 and 20MPa and at the temperature of between 1 and 80 DEG C; and performing secondary separation in the separation kettle with the stirrer under the pressure of between 4 and 8MPa and at the temperature ofbetween 1 and 85 DEG C, wherein the extraction and separation time is between 60 and 300 minutes, and the extraction rate of the borneol from the crude borneol is between 60 and 98 percent. The method replaces a conventional process for extracting, crystallizing and drying by using No.120 solvent gasoline, solves the problem of atmospheric pollution caused by the volatilization of the solvent gasoline, and eliminates tremendous potential safety hazard.

Description

technical field [0001] The present invention relates to borneol purification, particularly relates to, and the present invention particularly relates to utilizing supercritical CO 2 A method for separating borneol with a fluid extraction system with a stirred separation tank. Background technique [0002] Borneol is a synthetic drug in the Chinese Pharmacopoeia. At present, the method for synthesizing borneol is mainly under the catalysis of boric anhydride or metatitanic acid, and pinene and oxalate are esterified to generate bornyl oxalate, and then hydrolyzed with sodium hydroxide to generate crude borneol (solid, orthoborneol≤45%) ), no matter the kind of process route, the last thick borneol must use 120# solvent gasoline to dry to obtain the borneol product after twice crystallization and purification. Problems existing in the current process: first, gasoline is used as a solvent in the two crystallization and purification of crude borneol, and gasoline belongs to Cl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/30C07C29/76
CPCY02P20/54
Inventor 朱宝璋王伟冯志豪
Owner SOUTH CHINA UNIV OF TECH
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